CN114195184A - Preparation method and application of two-dimensional chalcogenide - Google Patents
Preparation method and application of two-dimensional chalcogenide Download PDFInfo
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- CN114195184A CN114195184A CN202210026015.XA CN202210026015A CN114195184A CN 114195184 A CN114195184 A CN 114195184A CN 202210026015 A CN202210026015 A CN 202210026015A CN 114195184 A CN114195184 A CN 114195184A
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- C—CHEMISTRY; METALLURGY
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- C01G19/006—Compounds containing, besides tin, two or more other elements, with the exception of oxygen or hydrogen
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
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Abstract
The invention discloses a two-dimensional chalcogenide, which is a crystalline material and has a chemical formula of (NH)4)2[Sn3S7]·(C4H13N3)1.41The unit cell parameters are:
α ═ β ═ 90 °, γ ═ 120 °, space group P63And/mmc. The invention also discloses a preparation method of the two-dimensional chalcogenide and application of the two-dimensional chalcogenide in iodine vapor adsorption. The disclosed two-dimensional chalcogenides are capable of operating at different concentrations of iodine vapor (as low as 400ppm) and at relatively wide temperaturesThe iodine vapor can be removed within the range (25-75 ℃) without desorption of iodine caused by long-time standing.
Description
Technical Field
The invention relates to the technical field of adsorption materials, in particular to a preparation method and application of a two-dimensional chalcogenide.
Background
Nuclear energy is one of the most promising clean energy sources for humans in the future. However, with the continuous development of nuclear power, the reserves of the spent fuel are also increasing. The spent fuel, which contains non-fissile uranium-235, is recovered and reused, and a large amount of gaseous radioactive iodine is generated in the process (i.e., spent fuel reprocessing). Compared with solid radioactive waste, the gaseous radioactive iodine has high fluidity and is easy to migrate along with airflow, so that the pollution area is larger, and the serious harm to the ecological environment and the human health is easier to generate. Research on nuclear accidents such as Chernobeli and Fudao shows that radioactive iodine is a type of radionuclide with rapid propagation and great harm. Therefore, the adsorption and treatment of gaseous iodine in the exhaust gas of post-treatment plants has become an important research content for radioactive exhaust gas treatment. At present, people mainly use methods such as dry dust removal, liquid absorption, solid phase adsorption and the like to remove radioactive iodine in gas. The dry dedusting has low processing efficiency on radioactive gas, and is mainly used for treating radioactive aerosol. The liquid absorption process mainly comprises mercury washing, acid washing and alkali washing. Although the method has high absorption efficiency, a large amount of toxic mercuric nitrate or strong acid and strong alkali such as nitric acid, sodium hydroxide and the like are used, the operation and maintenance cost of equipment is high, and a large amount of radioactive waste liquid is easily generated. Solid phase adsorption is one of the important iodine removal methods, the most commonly used being silver-containing zeolites. Although silver-based zeolite has high iodine removal efficiency, the adsorption material is high in cost due to the large amount of silver, and certain environmental pollution is caused.
The current industrial solid phase adsorption method for capturing radioiodine relies mainly on the use of active silver (Ag) supported on various solid carriers as an adsorbent. Active silver (silver nano-particles/silver nano-clusters/silver ions) can convert radioactive iodine into solid AgI, which in turn removes the iodine. The greatest limitation of this adsorbent in practical use is the instability of the Ag-I bond (the bond energy between Ag-I is typically 66 kJ/mol). When the silver-based adsorbent loaded with iodine is further processed, unstable Ag-I bonds are easily broken under the influence of external conditions such as illumination, temperature and the like, and radioactive iodine is released again to cause radioactive pollution.
In addition, the conventional industrial method for treating and capturing the iodine compound is to impregnate organic amine such as triethylenediamine on activated carbon. Triethylene diamine is the most common impregnant used in activated carbon adsorbents to capture radioiodine species. Compared with other adsorbents, the active carbon impregnated by the triethylene diamine has excellent adsorption capacity and higher purification efficiency, and the process of capturing iodine is relatively simple. However, its drawbacks are also evident: (1) the adsorbent capacity decreases with increasing temperature; (2) organic amine is easy to sublimate, so that the iodine absorption efficiency of the impregnated carbon material is obviously reduced; (3) iodine adsorption is an exothermic process, and the organic amine lowers the ignition point of the impregnated carbon, exacerbating potential safety hazards.
The metal organic framework material and the covalent organic framework material are novel crystalline porous materials, and the diversity of the metal center and the ligand endows the crystalline porous materials with variable chemical properties, so that the materials are widely applied to the removal of radioactive iodine. However, the expensive price of organic ligands limits the practical application of such materials.
Disclosure of Invention
In order to solve the technical problems, the invention synthesizes a novel two-dimensional layered sulfide material which can realize the high-efficiency removal of iodine vapor.
The invention provides the following technical scheme:
the invention provides a two-dimensional chalcogenide, which is a crystalline material and has a chemical formula of (NH)4)2[Sn3S7]·(C4H13N3)1.41The unit cell parameters are:
α ═ β ═ 90 °, γ ═ 120 °, space group P63/mmc。
The invention also provides a preparation method of the two-dimensional chalcogenide, which comprises the following steps: reacting a tin source and a sulfur simple substance in diethylenetriamine at 150-180 ℃ to obtain the two-dimensional chalcogenide; wherein the molar ratio of the tin source to the elemental sulfur is 1: 1-5.
Further, since the reaction needs to be carried out under heating and the reaction time is long, it is preferable to carry out the reaction in a closed vessel in order to avoid a large amount of volatilization of diethylenetriamine.
In the invention, diethylenetriamine plays a role of a solvent and a template agent in the reaction, and ammonium ions generated after the reaction are finished exist in the pore channels of the two-dimensional chalcogenide compound to play a role of balancing interlayer charges. The amount of diethylenetriamine added is preferably such that the reaction product is immersed therein, and is generally 1/5 to 3/5 parts by volume of the reaction vessel.
Further, the tin source is a simple substance of tin or a tetravalent tin salt. The tin simple substance includes but is not limited to tin powder, tin particles and tin rods, and tin powder is preferred. The tetravalent tin salt is preferably tin tetrachloride.
Further, the elemental sulfur is preferably sublimed sulfur.
Further, the reaction time is 3-7 days.
Further, the molar ratio of the tin source to elemental sulfur is 3: 7.
The invention also provides the application of the two-dimensional chalcogenide in the adsorption of iodine vapor.
Two-dimensional chalcogenides (NH) of the invention4)2[Sn3S7]·(C4N3H13)1.41S in its molecular structure2-Can convert gaseous I2Reduction to I-And then Sn is passed through4+And I-Reaction to form SnI4Thereby realizing the adsorption of iodine vapor. And, the generated SnI4The properties are stable, and the desorption phenomenon of iodine caused by long-time standing can not occur.
Further, the iodine vapor is radioactive iodine vapor.
Further, the two-dimensional chalcogenide compound has an adsorption amount of 1.66g/g for iodine vapor at an iodine vapor concentration of 400ppm at 25 ℃ and an adsorption amount of 2.12g/g for iodine vapor at an iodine vapor concentration of 400ppm at 75 ℃.
Compared with the prior art, the invention has the beneficial effects that:
1. aiming at the problems of high cost and limited radioactive iodine adsorption amount in spent fuel tail gas of the traditional silver-based zeolite material, the invention synthesizes a novel two-dimensional chalcogenide (NH)4)2[Sn3S7]·(C4H13N3)1.41Using S in the two-dimensional chalcogenide2-Will I2Reduction to I-And then Sn is passed through4+And I-Reaction to form SnI4Thereby realizing the adsorption of radioactive iodine vapor.
2. The two-dimensional chalcogenide compound can remove iodine vapor under different iodine vapor concentrations (as low as 400ppm) and in a wider temperature range (25-75 ℃), and does not cause the desorption phenomenon of iodine due to long-time standing.
3. The two-dimensional chalcogenide provided by the invention is low in cost, and the expected cost of the material required for adsorbing 1g of iodine vapor is only 0.4 yuan, so that the two-dimensional chalcogenide has the potential for developing industrial application.
Drawings
FIG. 1 is (NH)4)2[Sn3S7]·(C4H13N3)1.41Schematic structural diagram of (a);
FIG. 2 is(NH4)2[Sn3S7]·(C4H13N3)1.41In the structure (a), a triangular node is formed by a Sn atom and an S atom;
FIG. 3 is (NH)4)2[Sn3S7]·(C4H13N3)1.41Thermogravimetric analysis of (a);
FIG. 4(a) is a graph showing (NH) at 75 ℃4)2[Sn3S7]·(C4H13N3)1.41A graph showing the change of the adsorption amount of iodine vapor having a high concentration with time;
FIG. 4(b) shows (NH) adsorbed with iodine4)2[Sn3S7]·(C4H13N3)1.41Change chart of adsorption amount after long-time standing;
FIG. 5 is a graph of (NH) at 25 ℃ and 75 ℃4)2[Sn3S7]·(C4H13N3)1.41Equilibrium adsorption capacity for low concentration iodine vapor.
Detailed Description
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The experimental methods used in the following examples are conventional methods unless otherwise specified, and materials, reagents and the like used therein are commercially available without otherwise specified.
Example 1: synthesis of two-dimensional chalcogenides (NH)4)2[Sn3S7]·(C4H13N3)1.41
Adding 3mmol of tin powder and 7mmol of sulfur powder into a reaction container, adding 4mL of diethylenetriamine, sealing the reaction container, setting the reaction temperature at 180 ℃, reacting for 4 days, and carrying out programmed cooling for 12 hours to room temperature. After the reaction was complete, the reaction product was washed with water to give yellow crystals, designated SCU-SnS.
The obtained yellow crystals were subjected to an X-ray single crystal diffraction test, and the crystallographic parameters thereof are shown in Table 1.
TABLE 1 two-dimensional chalcogenides (NH)4)2[Sn3S7]·(C4H13N3)1.41Crystallographic parameters of
Fig. 1-2 are schematic structural views of two-dimensional chalcogenides. As can be seen from the figure, Sn atom and S atom form a node similar to a triangle, the nodes are connected with each other through the S atom to form a layered structure, layers are stacked to form a negatively charged framework structure, and ammonium ions exist in (NH)4)2[Sn3S7]·(C4H13N3)1.41The channel of (2) plays a role of balancing charges.
The obtained two-dimensional chalcogenide was subjected to thermogravimetric Testing (TG) performed in a nitrogen atmosphere at a temperature ranging from 30 ℃ to 900 ℃ at a temperature rise rate of 10 ℃/min, and the results are shown in fig. 3.
As can be seen from fig. 3, the two-dimensional chalcogenide can be stabilized at 200 ℃ under a nitrogen atmosphere, which indicates that the material has good thermal stability. The mass reduction between 30 ℃ and 100 ℃ is mainly caused by the volatilization of water molecules on the surface of SCU-SnS, and the structure collapses around 200 ℃.
Example 2
The two-dimensional chalcogenide material was placed in an atmosphere of iodine vapor (16000ppm) at a high concentration at 75 c, and the amount of iodine vapor adsorbed by the material was measured at intervals of time, and the results are shown in fig. 4 (a).
As can be seen from FIG. 4(a), with the increasing reaction time, the adsorption amount of iodine by the material gradually becomes gentle after rapidly increasing, and finally reaches an equilibrium value, and the adsorption amount reaches 6.12g/g, which is the currently reported inorganic material with the highest adsorption capacity.
Example 3
The two-dimensional chalcogenide material having iodine adsorbed thereon was left to stand, and changes in the amount of adsorption of iodine by the material were measured at intervals of time, and the results were shown in fig. 4 (b).
As can be seen from fig. 4(b), the iodine-adsorbed two-dimensional chalcogenide material still has a retention of iodine on the material of nearly 100% after standing for 6 days. This shows that the two-dimensional chalcogenide material does not cause desorption of iodine due to long-term standing and has good adsorption stability.
Example 4
The equilibrium adsorption of iodine vapor by the two-dimensional chalcogenide material was tested at 25 c and 75 c, respectively, in an atmosphere of 400ppm iodine vapor (near the concentration of iodine vapor during spent fuel reprocessing), and the results are shown in figure 5.
The result shows that the material has the adsorption capacity of 1.66g/g for iodine vapor under the conditions of 25 ℃ and the concentration of 400ppm of iodine vapor, and has the adsorption capacity of 2.12g/g for iodine vapor under the conditions of 75 ℃ (close to the temperature of the tail end of the spent fuel after-treatment tail gas device) and the concentration of 400ppm of iodine vapor.
In summary, the present invention provides novel two-dimensional chalcogenides (NH)4)2[Sn3S7]·(C4H13N3)1.41Has good adsorption effect on iodine vapor, does not cause desorption phenomenon of iodine due to long-time standing, and can be appliedRemoval of radioactive iodine vapor during spent fuel reprocessing.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (10)
1. A two-dimensional chalcogenide, wherein said two-dimensional chalcogenide is a crystalline material having the formula (NH)4)2[Sn3S7]·(C4H13N3)1.41The unit cell parameters are:
α ═ β ═ 90 °, γ ═ 120 °, space group P63/mmc。
2. The method of preparing a two-dimensional chalcogenide compound according to claim 1, comprising the steps of: reacting a tin source and a sulfur simple substance in diethylenetriamine at 150-180 ℃ to obtain the two-dimensional chalcogenide; wherein the molar ratio of the tin source to the elemental sulfur is 1: 1-5.
3. The method of preparing a two-dimensional chalcogenide compound according to claim 2, wherein said reaction is performed in a sealed environment.
4. The method of preparing a two-dimensional chalcogenide compound according to claim 2, wherein said tin source is tin powder or tin tetrachloride.
5. The method of producing a two-dimensional chalcogenide according to claim 2, wherein the elemental sulfur is sublimed sulfur.
6. The method of claim 2, wherein the molar ratio of the tin source to elemental sulfur is 3: 7.
7. The method of claim 2, wherein the reaction time is 3 to 7 days.
8. Use of the two-dimensional chalcogenide of claim 1 for adsorbing iodine vapor.
9. Use according to claim 8, wherein the iodine vapor is radioactive iodine vapor.
10. The use of claim 8, wherein said two-dimensional chalcogenide exhibits an adsorption capacity of 1.66g/g for iodine vapor at a concentration of 400ppm iodine vapor at 25 ℃ and an adsorption capacity of 2.12g/g for iodine vapor at a concentration of 400ppm iodine vapor at 75 ℃.
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| US3933688A (en) * | 1974-07-12 | 1976-01-20 | Exxon Research And Engineering Company | Method for lithiating metal chalcogenides and intercalated products thereof |
| US20130252798A1 (en) * | 2012-03-21 | 2013-09-26 | National Tsing Hua University | Metallic sulfide photocatalyst for carbon dioxide reduction and the preparation for the same |
| CN104399538A (en) * | 2014-09-24 | 2015-03-11 | 中国科学院福建物质结构研究所 | Compound, preparation method and application thereof as ion exchange material |
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| CN105754584B (en) * | 2016-04-08 | 2018-08-24 | 苏州大学 | The preparation method and applications of metal chalcogenide compound multifunctional nano probe |
| AU2018282493A1 (en) * | 2018-12-21 | 2020-07-09 | Monash University | CZTS precursor inks and methods for preparing CZTS thin films and CZTS-based devices |
| CN113351186B (en) * | 2021-06-18 | 2022-12-27 | 海南希源化工科技有限公司 | Preparation method of iodine adsorbent, obtained product and application |
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- 2021-12-28 WO PCT/CN2021/141923 patent/WO2023070930A1/en unknown
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| US3933688A (en) * | 1974-07-12 | 1976-01-20 | Exxon Research And Engineering Company | Method for lithiating metal chalcogenides and intercalated products thereof |
| US20130252798A1 (en) * | 2012-03-21 | 2013-09-26 | National Tsing Hua University | Metallic sulfide photocatalyst for carbon dioxide reduction and the preparation for the same |
| CN104399538A (en) * | 2014-09-24 | 2015-03-11 | 中国科学院福建物质结构研究所 | Compound, preparation method and application thereof as ion exchange material |
| CN105080623A (en) * | 2015-08-14 | 2015-11-25 | 中国科学院福建物质结构研究所 | Ion exchanger for separating and/or extracting rare earth elements |
| CN107952489A (en) * | 2017-12-12 | 2018-04-24 | 淮北师范大学 | A kind of synthetic method of organic inorganic hybridization photochemical catalyst |
| CN111135875A (en) * | 2019-12-20 | 2020-05-12 | 中国科学院福建物质结构研究所 | Composite ion exchanger, preparation method and application thereof |
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